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Journal of the Korean Chemical Society (JKCS)

ISSN 1017-2548(Print)
ISSN 2234-8530(Online)
Volume 39, Number 7
JKCSEZ 39(7)
February 20, 1995 

 
Title
Synthesis and Characterization of Tetranuclear Molybdenum(Ⅵ) Complexes with Butylamidoxime Derivatives

부틸아미드옥심 유도체의 몰리브덴(Ⅵ) 사핵 착물의 합성과 성질
Author
Soo-Gyun Roh, Sang Oh Oh*

노수균, 오상오*
Keywords
Abstract
배위자인 이소부틸, 노르말 부틸 및 메틸티오아세트아미드옥심과 출발 물질인 단핵 및 다핵 착물과의 반응에서 X2[Mo4O12{R'C(NH2)NO)2](X=n-Bu4N+, R'=(CH3)2CH, CH3CH2CH2, CH3SCH2; X=(CH3)2CHC(=NH2)NH2+, R'=(CH3)2CH; X=CH3CH2CH2C(=NH2)NH2+, R'= CH3CH2CH2; X=CH3SCH2C(=NH2)NH2+, R'=CH3SCH2)을 합성하였다. 합성한 착물은 원소분석, 적외선 및 핵자기공명에 의해 구조를 규명하였다. 얻은 착물중 {(CH3)2CHC(=NH2)2}2[Mo4O12{(CH3)2CHC(NH2)NO}2]은 X-선 단결정 회절에서 결정구조를 밝혔고, 얻은 데이타는 Monoclinic, P21/c, a=10.168(3)Å, b=11.768(1)Å, c=13.557(1)Å, β=102.08(1)°, V=1586.2(5)Å3, Z=2 이었고, 회절강도 2951개(Fo > 3s(Fo))에 대한 최종 신뢰도 인자는 0.026이었다. 이 착물의 구조는 평면상의 환형[MOⅥ4(μ-O)4)]과 두 개의 μ4-아미드옥시메이트로 구성되어 있다.

The tetranuclear complexes, X2[Mo4O12{R'C(NH2)NO)2] {X=n-Bu4N+, R'=(CH3)2CH, CH3CH2CH2, CH3SCH2; X=(CH3)2CHC(=NH2)NH2+, R'=(CH3)2CH; X=CH3CH2CH2C(=NH2)NH2+, R'= CH3CH2CH2; X=CH3SCH2C(=NH2)NH2+, R'=CH3SCH2} have been synthesized by the reactions of monomeric and polynuclear complexes with isobutyl-, butyl- and thiomethylacetamidoxime. The prepared complexes were identified by elemental analysis, infrared, 1H NMR and 13C NMR spectroscopy. The structure of complex {(CH3)2CHC(=NH2)NH2}2[Mo4O12{(CH3)2CHC(NH2)NO}2] was determined by X-ray single crystal diffraction. Crystal data are follows: Monoclinic, P21/c, a=10.168(3)Å, b=11.768(1)Å, c=13.557(1)Å, β=102.08(1)°, V=1586.2(5)Å3, Z=2, final R=0.026 for 2951(Fo > 3s(Fo)). This complex is composed of a planar cyclic [MOⅥ4(μ-O)4)] and two μ4-amidoximate.

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552 - 558
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